CN110193327A - The non-aqueous monoisopropanolamine that catalyzes and synthesizes is from separator and its technique - Google Patents
The non-aqueous monoisopropanolamine that catalyzes and synthesizes is from separator and its technique Download PDFInfo
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- CN110193327A CN110193327A CN201910610736.3A CN201910610736A CN110193327A CN 110193327 A CN110193327 A CN 110193327A CN 201910610736 A CN201910610736 A CN 201910610736A CN 110193327 A CN110193327 A CN 110193327A
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- monoisopropanolamine
- reactor
- separator
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- separator tube
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/89—Silicates, aluminosilicates or borosilicates of titanium, zirconium or hafnium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/0242—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid flow within the bed being predominantly vertical
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
- C07C213/04—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton by reaction of ammonia or amines with olefin oxides or halohydrins
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
- B01J2229/10—After treatment, characterised by the effect to be obtained
- B01J2229/18—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself
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- Chemical Kinetics & Catalysis (AREA)
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- Fluid Mechanics (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of monoisopropanolamine production technologies, and in particular to the non-aqueous monoisopropanolamine that catalyzes and synthesizes of one kind is from separator and its technique.The non-aqueous monoisopropanolamine that catalyzes and synthesizes is from separator, including reactor, propylene oxide import and ammonia imports are arranged in reactor head, discharge port is arranged in reactor lower part, inside reactor sets gradually abacus, porcelain ball and solid catalyst from bottom to top, is provided with collet outside reactor, discharge port is connected with separator tube, it is provided with cooling coil outside separator tube, valve A and valve B are provided on separator tube；The present invention also provides its techniques.Successive reaction may be implemented in described device, only produces monoisopropanolamine product, only forms considerably less diisopropanolamine (DIPA) and triisopropanolamine, and the requirement of monoisopropanolamine industrial goods can be met by not needing progress later separation；Technique of the present invention using the device, it is scientific and reasonable, simple and easy.
Description
Technical field
The present invention relates to a kind of monoisopropanolamine production technologies, and in particular to one kind is non-aqueous to catalyze and synthesize monoisopropanolamine certainly
Separator and its technique.
Background technique
The one kind of isopropanolamine as hydramine substance can be used for petroleum except sulfur additives, surfactant, emulsifier etc.
Industry has more excellent performance relative to other hydramine substances (ethanol amine), and not will cause secondary pollution.Isopropyl
Hydramine includes monoisopropanolamine (MIPA), diisopropanolamine (DIPA) (DIPA) and triisopropanolamine (TIPA).
Monoisopropanolamine, also known as 1- amino -2- propyl alcohol, soluble easily in water and ethyl alcohol.MIPA toxicity is very weak, but contains in its structure
There is amido, so having a degree of damage to eye and skin.The purposes of MIPA is very extensive: good lipid solubilization,
Foaming characteristic and foam stability are usually applied to compound probability detergent due to this unique property；It can be with
Thioglycolic acid reaction, products obtained therefrom can be used as cosmetic material.MIPA is because having hygroscopicity and alkalescent to be used as surface
Raw material, refining agent of activating agent etc.；Since its phosphoric acid salt substance and nitrite substance have good oxidation resistance, therefore
It is applied to lubricating oil and the antioxidant of other oils；Its special construction can also be anti-with acid and letones
It answers, reaction product can be used as emulsifier, solvent and plasticizer class substance.Isopropanolamine has good solvability, special
It is not that the substances such as the waste residue oil of petroleum refining, kerosene are put together to mix and be stirred by hydrocarbons with isopropanolamine and oleic acid
It mixes, more stable emulsion can be obtained.Meanwhile can also be reacted with fatty acid, the salts substances of generation are a kind of stabilizations
The good emulsifier of property is very good for the emulsifying effectiveness of vinylacetate.
Currently, the main method of production MIPA is directly to be reacted to obtain MIPA, DIPA, TIPA tri- with ammonium hydroxide and propylene oxide
The mixture of person, this mixture respectively obtain pure MIPA, DIPA and TIPA, meeting in production process using rectification under vacuum
Generate DIPA and TIPA simultaneously, when use must carry out later separation, operate very cumbersome.
It is domestic mainly to be produced using low concentration ammonia water law, need to slough the water in product in the processing after generating product, this
A large amount of energy will be consumed.High-pressure process and supercritical methanol technology all carry out under high pressure, pressure 15MPa or more, hypertonia, to equipment
Requirement with regard to particularly severe, which limits the large-scale application of High-pressure supercritical method at home, and domestic seldom non-aqueous urge
The report that agent catalysis propylene oxide is reacted with ammonia.Therefore, to overcome the shortcomings of domestic production technique, a kind of activity is found
Height is easily isolated, reusable, and the catalyst of the good catalysis propylene oxide open loop petrohol amine of selectivity is to domestic different
Propanolamine industry has great importance.
Summary of the invention
According to the above-mentioned deficiencies in the prior art, non-aqueous catalyzing and synthesizing monoisopropanolamine the object of the present invention is to provide a kind of
From separator, successive reaction is may be implemented in described device, is only produced monoisopropanolamine product, is only formed considerably less diisopropyl
Hydramine and triisopropanolamine, the requirement of monoisopropanolamine industrial goods can be met by not needing progress later separation；The present invention is simultaneously
Its technique is provided, it is scientific and reasonable, simple and easy.
The technical solution adopted by the present invention to solve the technical problems is:
For the non-aqueous monoisopropanolamine that catalyzes and synthesizes from separator, including reactor, epoxy is arranged in reactor head
Discharge port is arranged in propane import and ammonia imports, reactor lower part, and inside reactor sets gradually abacus, porcelain ball from bottom to top
And solid catalyst, collet is provided with outside reactor, and discharge port is connected with separator tube, and cooler pan is provided with outside separator tube
It manages, is provided with valve A and valve B on separator tube.
Wherein:
The reactor head is additionally provided with temperature measuring device and device for pressure measurement.
It is of the present invention non-aqueous to catalyze and synthesize technique of the monoisopropanolamine from separator, the specific steps are as follows:
1) solid catalyst is fitted into reactor, is warming up to 140-200 DEG C, led to nitrogen 10-15 minutes；
2) pass through propylene oxide import and ammonia imports are continuously passed through propylene oxide into reactor and ammonia is reacted,
The molar ratio of ammonia and propylene oxide is 1-10:1, the flow of ammonia: 80-100mL/min；
3) the temperature control of separator tube is 60-80 DEG C, and the monoisopropanolamine for reacting generation is produced from separator tube end, reaction
In the process, valve A is opened, and valve B is closed, and when producing product, valve A is closed, and valve B is opened.
The reaction velocity 600-800h reacted above-1, residence time 20-40s.
The boiling point of monoisopropanolamine product is 161 DEG C, and the boiling point of propylene oxide is 34 DEG C, and the temperature of separator tube is 60-80
DEG C, liquefied only monoisopropanolamine product occurs in separator tube, propylene oxide gas continues instead back to reaction zone
Answer, propylene oxide will not liquefy from beginning to end, further generate diisopropanolamine (DIPA) and triisopropanolamine chance it is micro- its
Only liquefied monoisopropanolamine product that is micro-, being produced from the bottom of separator tube.
Wherein:
The solid catalyst is the loaded modified Titanium Sieve Molecular Sieve of metal ion, metal ion be chromium ion and cobalt from
The load capacity of son, chromium ion and cobalt ions is 0.05-0.5%.
The solid catalyst the preparation method is as follows:
1) Titanium Sieve Molecular Sieve synthesizes
Using ethyl orthosilicate as silicon source, using butyl titanate as titanium source, using tetrapropylammonium hydroxide as template, with
SiO2·aTPAOH·bTiO2·cH2O forms gel, wherein 0 < a < 0.4,0 <b < 0.03；
Under agitation, it is mixed water, ethyl orthosilicate, butyl titanate and with tetrapropylammonium hydroxide, at 80 DEG C
Water bath with thermostatic control is stirred 24-30 hours, and deionized water is supplemented in whipping process to maintain forming for mixed liquor；
Mixed liquor is fitted into the stainless steel autoclave for having and claiming in polytetrafluoroethylene (PTFE), the crystallization 2-7 at 150-200 DEG C
It, the resulting powder of crystallization is washed to neutral and drying, resistance furnace internal program is then placed in and is warming up to 560-580 DEG C of roasting 5-
10 hours, it is cooled to room temperature, obtains Titanium Sieve Molecular Sieve；
2) loaded metal ion
It is impregnated using vacuum equi-volume impregnating, maceration extract is chromium nitrate solution and cobalt chloride solution, dip time
It is 8-10 hours, is dried at 120-140 DEG C after the completion of dipping, is roasted 3-4 hours at 600-620 DEG C, obtain solid catalyst.
Compared with prior art, the beneficial effects of the present invention are:
1, apparatus structure of the present invention is simple, design rationally, may be implemented successive reaction, in reaction process, only produce
Monoisopropanolamine product only forms considerably less diisopropanolamine (DIPA) and triisopropanolamine, and not needing progress later separation can expire
The requirement of sufficient monoisopropanolamine industrial goods.
2, the boiling-point difference of technology utilization monoisopropanolamine and propylene oxide of the present invention, realizes propylene oxide and liquid
Reaction system is left after ammonia continuous feed, only product monoisopropanolamine liquefaction, there was only minimal amount of diisopropanolamine (DIPA) in product
And triisopropanolamine, subsequent rectification under vacuum separation is not needed, the requirement of monoisopropanolamine industrial goods can be met.
3, the present invention also provides a kind of for synthesizing the solid catalyst of monoisopropanolamine, and the catalyst is to an isopropanol
The selectivity of amine product is good, further reduces the generation of diisopropanolamine (DIPA) and triisopropanolamine, has ensured in subsequent step not
It needs further to separate.
4, technique of the present invention, it is scientific and reasonable, simple and easy.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of apparatus of the present invention；
In figure: 1, reactor；2, propylene oxide import；3, ammonia imports；4, discharge port；5, orifice plate；6, porcelain ball；7, solid
Catalyst；8, collet；9, separator tube；10, cooling coil；11, valve A；12, valve B.
Specific embodiment
The embodiment of the present invention is described further with reference to the accompanying drawing:
Catalyst used in the examples is the loaded modified Titanium Sieve Molecular Sieve of metal ion, and metal ion is chromium ion and cobalt
The load capacity of ion, chromium ion and cobalt ions is 0.5% (corresponding embodiment 1), and 0.3% (corresponding embodiment 2), 0.1% is (right
Answer embodiment 3).
The solid catalyst the preparation method is as follows:
1) Titanium Sieve Molecular Sieve synthesizes
Using ethyl orthosilicate as silicon source, using butyl titanate as titanium source, using tetrapropylammonium hydroxide as template, with
SiO2·aTPAOH·bTiO2·cH2O forms gel, wherein a=0.2, b=0.02；
Under agitation, it is mixed water, ethyl orthosilicate, butyl titanate and with tetrapropylammonium hydroxide, at 80 DEG C
Water bath with thermostatic control is stirred 30 hours, and deionized water is supplemented in whipping process to maintain forming for mixed liquor；
Mixed liquor is fitted into in the stainless steel autoclave claimed in polytetrafluoroethylene (PTFE), crystallization 5 days at 200 DEG C will be brilliant
Change resulting powder to wash to neutral and drying, is then placed in resistance furnace internal program and is warming up to 560 DEG C of roastings 8 hours, be cooled to room
Temperature obtains Titanium Sieve Molecular Sieve；
2) loaded metal ion
It is impregnated using vacuum equi-volume impregnating, maceration extract is chromium nitrate solution and cobalt chloride solution, dip time
It is 10 hours, is dried at 130 DEG C after the completion of dipping, is roasted 4 hours at 600 DEG C, obtain solid catalyst.
Embodiment 1
As shown in Figure 1, the non-aqueous monoisopropanolamine that catalyzes and synthesizes is from separator, including reactor 1, reactor 1
Top is arranged propylene oxide import 2 and ammonia imports 3, and 1 lower part of reactor is arranged discharge port 4, inside reactor 1 from bottom to top according to
Secondary setting abacus 5, porcelain ball 6 and solid catalyst 7 are provided with collet 8 outside reactor 1, and discharge port 4 is connected with separator tube 9,
It is provided with cooling coil 10 outside separator tube 9, valve A11 and valve B12 are provided on separator tube 9.
Temperature measuring device and device for pressure measurement are additionally provided at the top of the reactor 1.
It is described non-aqueous to catalyze and synthesize technique of the monoisopropanolamine from separator, the specific steps are as follows:
1) solid catalyst is fitted into reactor, is warming up to 180 DEG C, led to nitrogen 12 minutes；
2) pass through propylene oxide import and ammonia imports are continuously passed through propylene oxide into reactor and ammonia is reacted,
The molar ratio of ammonia and propylene oxide is 10:1, the flow of ammonia: 100mL/min；
3) the temperature control of separator tube is 60 DEG C, and the monoisopropanolamine for reacting generation is produced from separator tube end, is reacted
Cheng Zhong, valve A are opened, and valve B is closed, and when producing product, valve A is closed, and valve B is opened.
The purity of the monoisopropanolamine product of extraction is 99.8%.
Embodiment 2
The structure of described device is the same as embodiment 1.
It is described non-aqueous to catalyze and synthesize technique of the monoisopropanolamine from separator, the specific steps are as follows:
1) solid catalyst is fitted into reactor, is warming up to 200 DEG C, led to nitrogen 10 minutes；
2) pass through propylene oxide import and ammonia imports are continuously passed through propylene oxide into reactor and ammonia is reacted,
The molar ratio of ammonia and propylene oxide is 5:1, the flow of ammonia: 80mL/min；
3) the temperature control of separator tube is 60 DEG C, and the monoisopropanolamine for reacting generation is produced from separator tube end, is reacted
Cheng Zhong, valve A are opened, and valve B is closed, and when producing product, valve A is closed, and valve B is opened.
The purity of the monoisopropanolamine product of extraction is 98.5%.
Embodiment 3
The structure of described device is the same as embodiment 1.
It is described non-aqueous to catalyze and synthesize technique of the monoisopropanolamine from separator, the specific steps are as follows:
1) solid catalyst is fitted into reactor, is warming up to 140 DEG C, led to nitrogen 15 minutes；
2) pass through propylene oxide import and ammonia imports are continuously passed through propylene oxide into reactor and ammonia is reacted,
The molar ratio of ammonia and propylene oxide is 1:1, the flow of ammonia: 90mL/min；
3) the temperature control of separator tube is 60 DEG C, and the monoisopropanolamine for reacting generation is produced from separator tube end, is reacted
Cheng Zhong, valve A are opened, and valve B is closed, and when producing product, valve A is closed, and valve B is opened.
The purity of the monoisopropanolamine product of extraction is 97.1%.
Comparative example
With embodiment 1, difference is that catalyst is H-MOR (Si/Al=for described device and technique and its reaction condition
7.5) zeolite.
The purity of its monoisopropanolamine product produced is 90.2%.
Claims (5)
1. a kind of non-aqueous monoisopropanolamine that catalyzes and synthesizes is from separator, it is characterised in that: including reactor (1), reactor (1)
Propylene oxide import (2) and ammonia imports (3) are arranged in top, and discharge port (4) are arranged in reactor (1) lower part, and reactor (1) is internal
Abacus (5), porcelain ball (6) and solid catalyst (7) are set gradually from bottom to top, are provided with collet (8) outside reactor (1),
Discharge port (4) is connected with separator tube (9), is provided with cooling coil (10) outside separator tube (9), separator tube is provided with valve on (9)
Door A (11) and valve B (12).
2. the non-aqueous monoisopropanolamine that catalyzes and synthesizes according to claim 1 is from separator, it is characterised in that: described is anti-
It answers and is additionally provided with temperature measuring device and device for pressure measurement at the top of device (1).
3. it is a kind of using it is described in claim 1 it is non-aqueous catalyze and synthesize technique of the monoisopropanolamine from separator, feature exists
In: specific step is as follows:
1) solid catalyst (7) is fitted into reactor (1), is warming up to 140-200 DEG C, led to nitrogen 10-15 minutes；
2) it is continuously passed through propylene oxide into reactor (1) by propylene oxide import (2) and ammonia imports (3) and ammonia carries out
The molar ratio of reaction, ammonia and propylene oxide is 1-10:1, the flow of ammonia: 80-100mL/min；
3) the temperature control of separator tube (9) is 60-80 DEG C, and the monoisopropanolamine for reacting generation is produced from separator tube (9) end, instead
During answering, valve A (11) is opened, and valve B (12) is closed, and when producing product, valve A (11) is closed, and valve B (12) is opened.
4. technique according to claim 3, it is characterised in that: the solid catalyst (7) is that metal ion load changes
Property Titanium Sieve Molecular Sieve, metal ion is chromium ion and cobalt ions, and the load capacity of chromium ion and cobalt ions is 0.05-0.5%.
5. technique according to claim 3, it is characterised in that: the solid catalyst (7) the preparation method is as follows:
1) Titanium Sieve Molecular Sieve synthesizes
Using ethyl orthosilicate as silicon source, using butyl titanate as titanium source, using tetrapropylammonium hydroxide as template, with
SiO2·aTPAOH·bTiO2·cH2O forms gel, wherein 0 < a < 0.4,0 <b < 0.03；
Under agitation, it is mixed water, ethyl orthosilicate, butyl titanate and with tetrapropylammonium hydroxide, constant temperature at 80 DEG C
Stirring in water bath 24-30 hours, deionized water is supplemented in whipping process to maintain forming for mixed liquor；
Mixed liquor is fitted into in the stainless steel autoclave claimed in polytetrafluoroethylene (PTFE), crystallization 2-7 days at 150-200 DEG C will
The resulting powder of crystallization is washed to neutral and dry, and being then placed in resistance furnace internal program, to be warming up to 560-580 DEG C of roasting 5-10 small
When, it is cooled to room temperature, obtains Titanium Sieve Molecular Sieve；
2) loaded metal ion
It is impregnated using vacuum equi-volume impregnating, maceration extract is chromium nitrate solution and cobalt chloride solution, dip time 8-
It 10 hours, is dried at 120-140 DEG C after the completion of dipping, is roasted 3-4 hours at 600-620 DEG C, obtain solid catalyst.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910610736.3A CN110193327A (en) | 2019-07-08 | 2019-07-08 | The non-aqueous monoisopropanolamine that catalyzes and synthesizes is from separator and its technique |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910610736.3A CN110193327A (en) | 2019-07-08 | 2019-07-08 | The non-aqueous monoisopropanolamine that catalyzes and synthesizes is from separator and its technique |
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| CN110193327A true CN110193327A (en) | 2019-09-03 |
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| CN201910610736.3A Withdrawn CN110193327A (en) | 2019-07-08 | 2019-07-08 | The non-aqueous monoisopropanolamine that catalyzes and synthesizes is from separator and its technique |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114247470A (en) * | 2021-12-31 | 2022-03-29 | 南京红宝丽醇胺化学有限公司 | Preparation method of catalyst and synthesis method of monoisopropanolamine |
| CN114405430A (en) * | 2022-01-21 | 2022-04-29 | 华峰集团上海工程有限公司 | System and method for synthesizing isopropanolamine |
-
2019
- 2019-07-08 CN CN201910610736.3A patent/CN110193327A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114247470A (en) * | 2021-12-31 | 2022-03-29 | 南京红宝丽醇胺化学有限公司 | Preparation method of catalyst and synthesis method of monoisopropanolamine |
| CN114247470B (en) * | 2021-12-31 | 2024-07-12 | 南京红宝丽醇胺化学有限公司 | Preparation method of catalyst and synthesis method of monoisopropanolamine |
| CN114405430A (en) * | 2022-01-21 | 2022-04-29 | 华峰集团上海工程有限公司 | System and method for synthesizing isopropanolamine |
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Application publication date: 20190903 |